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Preparation method and application of cortex albiziae lignan glycoside monomers

A kind of technology of lignan glycosides and Albizia Julibrissin bark, which is applied in the field of preparation of lignan glucoside monomers of Albizia Julibrissin

Active Publication Date: 2018-09-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no documented research on extracting FAS-inhibiting monomers from the bark of Albizia Julibrissin

Method used

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  • Preparation method and application of cortex albiziae lignan glycoside monomers
  • Preparation method and application of cortex albiziae lignan glycoside monomers
  • Preparation method and application of cortex albiziae lignan glycoside monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Isolation and Purification of Lignan Glycoside Monomer (Acanthoside E1) from the Bark of Albizia Julibrissin

[0031] 2.5kg of Albizia Julibrissin medicinal material was crushed into powder, refluxed and extracted twice in 75% ethanol at 75°C, the ratio of solid to liquid was 1:10 (g / mL), and the refluxed extraction time was 2h. The two extracts were combined, concentrated under reduced pressure, and dried in vacuo to obtain 250 g of the total extract of Albizia Julibrissin (AJ-T), and the yield of the crude product was 10%. The total extract was dissolved in distilled water, and then fractionally extracted with ethyl acetate and water-saturated n-butanol, respectively. The extract was concentrated under reduced pressure to obtain an ethyl acetate phase (124.7 g), n-butanol phase AJ-B (52.4 g), and a mother liquor aqueous phase (23.5 g).

[0032] Take 20g of albizia juniper n-butanol dry powder, dissolve it in deionized water, elute the aqueous solution through a D101 ...

Embodiment 2

[0036] Structural identification of lignan glycoside monomer (eleutheroside E1) from the bark of Albizia Julibrissin

[0037] Sample H2 was dried, ground, and directly pressed into tablets with iodine bromide, detected by Fourier transform infrared spectrometer, and analyzed in the mid-infrared region (wavenumber 4000-400cm -1 ) change, record the infrared spectrum ( image 3 , the infrared spectrum of the sample), the IR spectrum results suggest that the compound contains a benzene ring, a carbon-oxygen bond or a hydroxyl group.

[0038] Mass Spectrometry Conditions: Ion Mode: ESI + ; Capillary voltage: 3.5kVolts; Cone voltage: 20Volts; Ion source temperature: 100℃; Desolvation temperature: 400℃; Mass range 100-1000m / z; Voltage: 1800Volts. MassLynx software was used to collect and process data, and the relative molecular mass of the compound was known to be 580. Multiple fragment ion peaks are generated simultaneously. ( Figure 4 , the mass spectrum of the sample)

[...

Embodiment 3

[0043] Detection of Fatty Acid Synthase Activity by UV-Vis Spectrophotometry

[0044] Fatty acid synthase supernatant was extracted and purified from chicken liver. NADPH has absorption at 340nm, but its product NADP has no absorption at 340nm. Therefore, the change of NADPH was determined by a microplate reader to determine the change of fatty acid synthase activity. Carried out in potassium phosphate buffer containing 1mmol / L EDTA, pH 7, concentration 0.1mmol / L, substrate concentration acetyl CoA 6μmol / L, malonyl CoA 12μmol / L, NADPH 37.5μmol / L, to be The concentration of the test sample is 50ug / mL, the total reaction volume is 2mL, after 4-5min in a 37°C water bath, add 50μL of diluted high-speed centrifuged fatty acid synthase supernatant to start the enzyme reaction, and absorb 200uL of the reaction system from the reaction system each time The solution was continuously monitored for changes in absorbance at a wavelength of 340 nm.

[0045] The activity unit (U) of anima...

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Abstract

The invention belongs to the technical field of traditional Chinese medicine, and particularly relates to a preparation method and application of cortex albiziae lignan glycoside monomers. Eleutheroside E1 monomers with the inhibition effects on fatty acid synthase are extracted and separated from traditional Chinese medical materials of cortex albiziae. The preparation process comprises the following steps of crushing the cortex albiziae into powder; performing ethanol backflow extraction; sequentially performing extraction by ethyl acetate and water saturated n-butyl alcohol; performing elution by macroporous resin; performing silica gel column chromatographic separation; performing semi-preparation efficient liquid phase separation, reduced pressure concentration and drying to obtain afinished product. The infrared spectroscopy, nuclear magnetic resonance technology and mass spectrum are used for determining the chemical structure. The method is simple and fast; the required solvents are few; the yield is higher; higher economic values and academic values are realized.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicines, and in particular relates to a preparation method and application of albizia juniper lignan glycoside monomer. Background technique [0002] Animal fatty acid synthase (Fatty acid synthase, FAS) is a key enzyme in the pathway of catalyzing the synthesis of long-chain fatty acids in animals, and is a multifunctional complex enzyme of energy metabolism. Studies have shown that FAS has been found in recent years to become a new dual potential target for weight loss and anti-cancer. The development of fatty acid synthase inhibitors with high activity and low toxicity is of great significance for the prevention and treatment of cancer. So far, there are very few FAS inhibitor monomers reported, only the earliest discovered natural product cerulenin (cerulenin) and C75 synthesized chemically using the structure of cerulenin as a template, and the ester type catechin in green tea ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08A61P35/00A61P3/04A23L33/105A61K8/60A61Q19/00
CPCA23L33/105A23V2002/00A61K8/602A61P3/04A61P35/00A61Q19/00C07H1/08C07H15/203A23V2200/30A23V2250/21A23V2300/14
Inventor 邱丽颖谭方根雷月月蔡维维孙海建龚蕾蕾李曰周跃涛侯豹朱雪雪高越颖胡静徐非
Owner JIANGNAN UNIV
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